Abstract: The Fe-Cr co-doped TiO2 nanosphere were synthesized with Titanium butoxide, Iron (III) nitrate nonahydrate, Chromium (III) nitrate nonahydrate by a modified sol-gel method. The crystal structure, morphology and optical absorption property of as-prepared nanosphere were characterized. And the photocatalytic hydrogen evolution was performed under UV-vis light illumination. It turned out that the Fe-Cr co-doped TiO2 nanosphere obtains the best photocatalytic hydrogen evolution activity (133.6 μmol/g/h) and also exhibits high reusability for photocatalytic reaction.